Two procedures for the determination of scandium in coal fly ash and other geological materials have been developed. The first procedure consists in dissolution of the samples with a mixture of nitric, perchloric and hydrofluoric acids in a sealed PTFE vessel followed by determination by graphite furnace atomic absorption spectrometry. In the second procedure, the sample is decomposed by fusion with lithium tetraborate, the melt is dissolved in 5% nitric acid and scandium is determined by inductively coupled plasma atomic emission spectrometry using an argon plasma. The limits of determination are 0.80 and 0.63 µg g^–1, respectively, for the two methods. The scandium concentration in eight coal ash samples obtained by GFAAS and ICP-AES compare well with those determined previously by NAA.